CN103073433A - Energy-saving recovery technology of 3-dimethylaminopropylamine (DMAPA) - Google Patents

Energy-saving recovery technology of 3-dimethylaminopropylamine (DMAPA) Download PDF

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Publication number
CN103073433A
CN103073433A CN2012105504528A CN201210550452A CN103073433A CN 103073433 A CN103073433 A CN 103073433A CN 2012105504528 A CN2012105504528 A CN 2012105504528A CN 201210550452 A CN201210550452 A CN 201210550452A CN 103073433 A CN103073433 A CN 103073433A
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CN
China
Prior art keywords
dmapa
energy
water
dimethylaminopropylamine
removal agent
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Pending
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CN2012105504528A
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Chinese (zh)
Inventor
雷小英
夏雄燕
徐浩
华文高
黄亚茹
邹焕金
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Jiaxing Zanyu Technology Co Ltd
ZHEJIANG ZANYU TECHNOLOGY Co Ltd
Original Assignee
Jiaxing Zanyu Technology Co Ltd
ZHEJIANG ZANYU TECHNOLOGY Co Ltd
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Priority to CN2012105504528A priority Critical patent/CN103073433A/en
Publication of CN103073433A publication Critical patent/CN103073433A/en
Pending legal-status Critical Current

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Abstract

The invention relates to an energy-saving recovery technology of DMAPA. The technology has the characteristics of energy consumption reduction, environmental protection benefiting, easy equipment making, and low production cost. A technical scheme adopted in the invention is characterized in that the energy-saving recovery technology of the DMAPA sequentially comprises the following steps: 1, allowing a DMAPA-water mixed solution from a condenser to enter a separator through a pipeline, adding a water removal agent through a feed inlet, stirring, and allowing the obtained mixture to stand for layering, wherein the addition amount of the water removal agent is 10-90% of the weight of the DMAPA-water mixed solution; 2, conveying the supernatant obtained in step 1 to a distillation kettle through a pipeline, carrying out reduced pressure distillation at a temperature of 60-140DEG C under a relative pressure of 0MPa - -0.085MPa, and collecting the obtained distillation condensate which is the DMAPA; and 3, discharging the lower-layer liquid obtained in step 1 from the material outlet at the bottom of the separator, wherein the lower-layer liquid is the aqueous solution of the water removal agent.

Description

A kind of energy-saving reclaiming process of 3-dimethylaminopropylamine
Technical field
The present invention relates to a kind of from 3-dimethylaminopropylamine (be called for short DMAPA) and water mixed solution the energy-saving technique of recovery DMAPA, described water mixed solution is the DMAPA that produces in cats product alkylamide propyl dimethyl tertiary amine production process and the mixing solutions of water.The production technique field that belongs to tensio-active agent.
Background technology
DMAPA density 0.8100g/cm 2, zero pour-70 ℃, 134 ℃ of boiling points, molecular weight 102 can water-soluble and organic solvent, has corrodibility, and eyes, mucous membrane, skin are had pungency, can cause human body and burn.DMAPA mainly as organic synthesis intermediate, is used for producing dyestuff, ion exchange resin; As epoxy curing agent, oil plant and cyanideless electro-plating zinc additive, fiber and leather treatment and sterilant etc.In the tensio-active agent industry, DMAPA is one of raw material of synthesizing cationic tensio-active agent alkylamide propyl dimethyl tertiary amine, and another raw material is lipid acid.Guarantee the transformation efficiency of lipid acid in the reaction, DMAPA is excessive to feed intake, the water that generates in excessive DMAPA and the reaction process, under 130 ~ 160 ℃ of reaction conditionss, from reactor, be evaporated, obtain the DMAPA waste liquid through the condenser condenses collection, contain 20~40% DMAPA, 60 ~ 80% water, 0.1 ~ 0.3% lipid acid, 0.1 ~ 0.3% alkylamide propyl dimethyl tertiary amine in the waste liquid, can not directly utilize.The DMAPA chemical property is active, has stronger volatility, toxicity, corrodibility, directly discharges the meeting serious environment pollution, and the environmental protection treatment cost is high again, more can cause wastage of material.The conventional processing scheme is to waste liquid multistage rectification Separation and Recovery DMAPA at present.(application number: the aqueous solution of two platen presses of 02822683.6) mainly having described the binary mixture that utilizes rectifying homogeneous phase azeotropic by continuous still battery amine is the method for separation of amine therefrom for the method for separation of amine from the aqueous solution; A kind of method of fractionation by distillation amine aqueous solution (application number: 200510075475.8) mainly describe the method for the distillation processing separation of amine aqueous solution of high energy efficiency, described method all needs to adopt the above rectifier unit of secondary to the recovery of amine, just can isolate highly purified amine, qualified discharge after the wastewater treatment.Multistage rectification device subject matter: construction investment is large, energy consumption is high, and cost recovery is higher than the value of waste liquid.Therefore, design DMAPA energy-saving waste liquid recovery technique has great importance to reduction product cost, minimizing discharging.
Summary of the invention
The objective of the invention is to overcome the deficiency that the above-mentioned background technology exists, a kind of energy-saving reclaiming process of 3-dimethylaminopropylamine is provided, this technique should have the characteristics that reduce energy consumption, are conducive to environment protection, and device fabrication is easy, production cost is low.
Technical scheme provided by the invention is: a kind of energy-saving reclaiming process of 3-dimethylaminopropylamine, carry out successively according to the following steps:
1) enters separator from condenser DMAPA water mixed solution out by pipeline, add water-removal agent by charging opening, standing demix after stirring; The water-removal agent add-on is 10~90% of DMAPA water mixed solution weight.
2) supernatant liquid is transported to still kettle by pipeline and carries out underpressure distillation, and the relative pressure of underpressure distillation is 0 ~-0.085MPa, the temperature during underpressure distillation is 60 ~ 140 ℃, the distillation phlegma DMAPA of collection.
3) lower floor's liquid is the water-removal agent aqueous solution, from the discharging of separator bottom discharge mouth.
Described water-removal agent is the mixture of one or more arbitrary proportions in inorganic salt or the mineral alkali.
The relative pressure of described underpressure distillation is-0.065 ~-0.080MPa.
As recommendation, the relative pressure of underpressure distillation is-0.065 ~-0.080MPa, the temperature of underpressure distillation is controlled at 80 ~ 90 ℃.
Described inorganic salt are mixtures of one or more arbitrary proportions in anhydrous sodium sulphate, anhydrous potassium sulfate, sodium-chlor, the Repone K.
Described mineral alkali is the mixture of one or more arbitrary proportions in calcium hydroxide, calcium oxide, magnesium hydroxide, magnesium oxide, sodium hydroxide, potassium hydroxide, sodium oxide, potassium oxide, sodium methylate, the potassium methylate.
Principle of the present invention is: according to the immiscible characteristics of the aqueous solution of water-removal agent and DMAPA, and the water among the water-removal agent absorption DMAPA of adding, the little upper strata that is distributed in of DMAPA density, liquid density is distributed in greatly lower floor after the water-removal agent suction; Upper strata DMAPA mixed solution through single flash, is removed the impurity of DMAPA, obtain transparent DMAPA.
The DMAPA that energy-saving reclaiming process provided by the invention is mainly used in the production of alkylamide propyl dimethyl tertiary amine reclaims.After described DMAPA water mixed solution separates, among the DMAPA that obtains water-content less than 3%, can direct reuse in the production of alkylamide propyl dimethyl tertiary amine, the lower floor's solution after the separation can be used for preparing industrial cleaning agent.The method has the advantages that separating device is easy to get, energy consumption is low.Compare with existing technique, following outstanding advantages and positively effect are arranged;
1, water-removal agent directly separates propylene diamine and the aqueous solution, and separating device is easily made, reduced investment.
2, remove impurity in the material by a underpressure distillation, need not multistage rectification, energy consumption descends and 30~60% reduces the DMAPA cost recovery.
3, DMAPA content in upper strata reaches more than 97%, can be used for the production of alkylamide propyl dimethyl tertiary amine or other application, and separating effect is better.
4, the aqueous solution of lower floor's water-removal agent can be used for industrial cleaning agent production, without discharging of waste liquid, does not have treatment cost of waste liquor, realizes minimizing of production process discharging.
5, whole technique easily realizes the pipeline conveying, reduces evaporating, emitting, dripping or leaking of liquid or gas, reduces and pollutes, and realizes cleaner production.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Among the figure: 1 condenser, 2 secondary charging mouths, 3 interface liquid level gauges, 4 separators, 5 hold-up vessel A, 6 still kettles, 7 hold-up vessel B.
Embodiment
Further specify below in conjunction with embodiment and accompanying drawing 1.
Technical process provided by the invention is: enter separator from condenser DMAPA solution out by pipeline, add water-removal agent by charging opening, standing demix after stirring.When the water content of supernatant liquid material≤3.0%, supernatant liquid is transported to still kettle by pipeline, carries out underpressure distillation, collects distillation phlegma DMAPA and enters hold-up vessel B, can be used for the production of alkylamide propyl dimethyl tertiary amine; Subnatant enters hold-up vessel A from separator bottom discharge mouth and can be used for industrial cleaning agent production.
Working process of the present invention is as shown in Figure 1:
Out the direct pipeline of the DMAPA aqueous solution is transported to separator 4 from condenser 1, adds water-removal agent by secondary charging mouth 2 in separator 4, and opens and stir, and stops to stir standing demix after fully until material dissolution; Check the situation of feed separation by the variation of interface liquid level gauge 3 liquid levels, when treating upper materials water content≤3.0%, upper strata DMAPA can be transported to still kettle 6 by discharge port; Still kettle 6 temperature are controlled at 60 ~ 140 ℃, and relative pressure is controlled at 0 ~-0.085Mpa, collect the DMAPA phlegma to hold-up vessel B, can be used for the production of alkylamide propyl dimethyl tertiary amine, isolated lower floor solution is transported to hold-up vessel A by lower discharge port.
Described relative pressure is the difference of still kettle internal pressure and barometric point, and negative value represents that the still kettle internal pressure is less than barometric point.
Described separator left upper end is with a secondary charging mouth 2, and upper right side is with interface liquid level gauge 3, and the separator both sides are with four discharge ports and a lower discharge port.
Described interface liquid level gauge 3 is the interfacial levels that show material according to material density.
Condenser of the present invention, secondary charging mouth, interface liquid level gauge, separator, hold-up vessel A, still kettle, the equal buyable of hold-up vessel B obtain.
Embodiment 1
Pump into the 720kgDMAPA aqueous solution (amine value 431.2mgKOH/g) in separator 4 from condenser 1, open and stir, from charging opening 2, add simultaneously solid sodium hydroxide 204kg and calcium hydroxide 5kg, check material state by the discharge port visor, after material dissolution is complete, stop to stir, leaving standstill approximately 2 hours, get upper materials from discharge port and measure the amine value, the amine value is 1059mgKOH/g, check the height of upper materials by interface liquid level gauge 3, upper strata DMAPA is transported to still kettle 6 by discharge port carries out underpressure distillation; To open simultaneously still kettle 6 heating, condensation and vacuum system, allow temperature of charge be controlled at 60 ~ 65 ℃, relative pressure is controlled at-0.065 ~-0.08MPa, collect approximately 293kg(content 98.3% of DMAPA phlegma).The DMAPA phlegma is delivered directly to storage tank B, can be used for producing the fatty amide propyl dimethyl tertiary amine; Isolated lower floor solution is 635kg approximately, is transported to hold-up vessel A by the direct pipeline of lower discharge port and is used in the cleaner production of industrial cleaning agent.
Embodiment 2
Enter the separator 4 by pipeline from condenser 1 579kg DMAPA solution (amine value 215.6mgKOH/g) out, directly add 158kg anhydrous chlorides of rase sodium in propylene diamine separating tank 4 by charging opening 2, stir about 1 hour, behind the standing demix, getting supernatant liquid mensuration amine value is 1063mgKOH/g; Check the height of upper materials by interface liquid level gauge 3, upper strata DMAPA is delivered to still kettle 6 by discharge port, open vacuum and heating system, material is warmed up to 80~85 ℃, relative pressure is controlled at-0.06 ~-0.07MPa, collect approximately 118kg(DMAPA content 98.6% of DMAPA phlegma); With the defeated storage tank B of the direct pipeline of DMAPA; The liquid 618kg of lower floor is transported to hold-up vessel A by the direct pipeline of lower discharge port.
Embodiment 3
Squeeze into separating tank 4 from the condenser 540kgDMAPA aqueous solution (amine value 323.4mgKOH/g) out, add 208kg potassium hydroxide from charging opening 2, stir about 1 hour, evenly rear standing demix, getting supernatant liquid mensuration amine value is 1057.5mgKOH/g; Check the height of upper materials by interface liquid level gauge 3, upper strata DMAPA is transported to still kettle 6 by right discharge port, material is warmed up to 70~75 ℃, relative pressure is controlled at-0.075 ~-0.08MPa, collect altogether approximately 165kg(DMAPA content 98.1% of DMAPA phlegma); The DMAPA phlegma is transported to hold-up vessel B; The liquid 582kg of lower floor is transported to hold-up vessel A by the direct pipeline of lower discharge port.
Embodiment 4
Squeeze into separating tank 4 from the condenser 620kgDMAPA aqueous solution (amine value 300.4mgKOH/g) out, add successively 150kg sodium oxide and 114kg sodium hydroxide from charging opening 2, stir about 1 hour, evenly rear standing demix, getting supernatant liquid mensuration amine value is 1051.0mgKOH/g; Check the height of upper materials by interface liquid level gauge 3, upper strata DMAPA is transported to still kettle 6 by right discharge port, material is warmed up to 70~75 ℃, relative pressure is controlled at-0.065 ~-0.085MPa, collect altogether approximately 177kg(DMAPA content 97.5% of DMAPA phlegma); DMAPA is transported to hold-up vessel B; The liquid 706kg of lower floor is transported to hold-up vessel A by the direct pipeline of lower discharge port.
Above-described embodiment is used for the present invention that explains, rather than limits the invention, and in the protection domain of spirit of the present invention and claim, any modification and change to the present invention makes all fall into protection scope of the present invention.

Claims (6)

1. the energy-saving reclaiming process of a 3-dimethylaminopropylamine, carry out successively according to the following steps:
1) enters separator (3) from condenser DMAPA water mixed solution out by pipeline, add water-removal agent by charging opening (4), standing demix after stirring; The water-removal agent add-on is 10~90% of DMAPA water mixed solution weight;
2) supernatant liquid is transported to still kettle (6) by pipeline and carries out underpressure distillation, and the relative pressure of underpressure distillation is 0 ~-0.085MPa, the temperature during underpressure distillation is 60 ~ 140 ℃; Collect distillation phlegma DMAPA.
3) lower floor's liquid is the water-removal agent aqueous solution, from the discharging of separator bottom discharge mouth.
2. the energy-saving reclaiming process of a kind of 3-dimethylaminopropylamine according to claim 1 is characterized in that described water-removal agent is the mixture of one or more arbitrary proportions in inorganic salt or the mineral alkali.
3. the energy-saving reclaiming process of a kind of 3-dimethylaminopropylamine according to claim 3, the relative pressure that it is characterized in that described underpressure distillation be-0.065 ~-0.080MPa.
4. the energy-saving reclaiming process of a kind of 3-dimethylaminopropylamine according to claim 4 is characterized in that the temperature of described underpressure distillation is controlled at 80 ~ 90 ℃.
5. the energy-saving reclaiming process of a kind of 3-dimethylaminopropylamine according to claim 5 is characterized in that described inorganic salt are mixtures of one or more arbitrary proportions in anhydrous sodium sulphate, anhydrous potassium sulfate, sodium-chlor, the Repone K.
6. the energy-saving reclaiming process of a kind of 3-dimethylaminopropylamine according to claim 6 is characterized in that described mineral alkali is the mixture of one or more arbitrary proportions in calcium hydroxide, calcium oxide, magnesium hydroxide, magnesium oxide, sodium hydroxide, potassium hydroxide, sodium oxide, potassium oxide, sodium methylate, the potassium methylate.
CN2012105504528A 2012-12-17 2012-12-17 Energy-saving recovery technology of 3-dimethylaminopropylamine (DMAPA) Pending CN103073433A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104478733A (en) * 2014-12-10 2015-04-01 九江天赐高新材料有限公司 Method for recycling bis-DMAPA from DMAPA heavy components
CN104557596A (en) * 2014-12-18 2015-04-29 广州花语精细化工有限公司 Method for treating N,N-dimethyl-1,3-propane diamine waste liquor

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0908444A2 (en) * 1997-10-07 1999-04-14 Kao Corporation A process for producing a tertiary amine having high quality
CN102026956A (en) * 2008-05-13 2011-04-20 巴斯夫欧洲公司 Method for producing N,N-substituted-1,3-propandiamines
CN102134202A (en) * 2011-01-31 2011-07-27 浙江赞宇科技股份有限公司 Technology for continuously producing alkyl amide propyl group betaine

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0908444A2 (en) * 1997-10-07 1999-04-14 Kao Corporation A process for producing a tertiary amine having high quality
CN102026956A (en) * 2008-05-13 2011-04-20 巴斯夫欧洲公司 Method for producing N,N-substituted-1,3-propandiamines
CN102134202A (en) * 2011-01-31 2011-07-27 浙江赞宇科技股份有限公司 Technology for continuously producing alkyl amide propyl group betaine

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104478733A (en) * 2014-12-10 2015-04-01 九江天赐高新材料有限公司 Method for recycling bis-DMAPA from DMAPA heavy components
CN104557596A (en) * 2014-12-18 2015-04-29 广州花语精细化工有限公司 Method for treating N,N-dimethyl-1,3-propane diamine waste liquor

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